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#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_7804

_audit_creation_method           SHELXL-97
_audit_creation_date             2012-05-11
_audit_block_code                WGT-CM-517-17
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H92 O32 S2 V8, 2(C16 H36 N)'
_chemical_formula_sum            'C92 H164 N2 O32 S2 V8'
_chemical_formula_weight         2281.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-p 2yn'
_symmetry_Int_Tables_number      14

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.1675(12)
_cell_length_b                   20.323(2)
_cell_length_c                   20.135(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.855(9)
_cell_angle_gamma                90.00
_cell_volume                     5760.5(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    181957
_cell_measurement_theta_min      2.6923
_cell_measurement_theta_max      33.0995

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 -1.00 0.1500
0.00 0.00 1.00 0.1500
1.00 0.00 -1.00 0.1300
-1.00 0.00 1.00 0.1300
0.00 -1.00 1.00 0.1100
0.00 1.00 -1.00 0.1100
1.00 0.00 3.00 0.1700

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2404
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_absorpt_correction_T_min  0.71712
_exptl_absorpt_correction_T_max  0.89215

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD φ- and ω-scans'
_diffrn_detector_area_resol_mean 18.02
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            164119
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.87
_diffrn_reflns_theta_max         33.07
_reflns_number_total             21758
_reflns_number_gt                15539
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0489P)²+9.2104P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         21758
_refine_ls_number_parameters     652
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0553
_refine_ls_wR_factor_ref         0.1411
_refine_ls_wR_factor_gt          0.1242
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.23715(2) 0.079238(18) 0.499157(18) 0.01580(7) Uani 1 1 d . . .
V2 V 0.01034(2) 0.114404(18) 0.400185(18) 0.01586(7) Uani 1 1 d . . .
V3 V 0.08697(3) 0.177203(18) 0.566825(19) 0.01716(7) Uani 1 1 d . . .
V4 V 0.10105(2) 0.027750(18) 0.568060(18) 0.01580(7) Uani 1 1 d . . .
O51 O 0.32885(10) 0.08038(8) 0.57167(8) 0.0208(3) Uani 1 1 d . . .
O52 O -0.06903(11) 0.11749(8) 0.32182(8) 0.0224(3) Uani 1 1 d . . .
O53 O 0.16635(12) 0.18697(9) 0.64471(8) 0.0238(3) Uani 1 1 d . . .
O54 O 0.17807(11) 0.02169(9) 0.64739(8) 0.0228(3) Uani 1 1 d . . .
O55 O 0.02545(10) -0.03700(7) 0.55968(8) 0.0176(3) Uani 1 1 d . . .
O56 O 0.12840(10) 0.10774(7) 0.51903(8) 0.0160(3) Uani 1 1 d . . .
O61 O 0.18219(10) -0.00452(8) 0.51726(8) 0.0175(3) Uani 1 1 d . . .
C62 C 0.24074(17) -0.06123(12) 0.54288(14) 0.0274(5) Uani 1 1 d . . .
H62A H 0.2866 -0.0528 0.5914 0.041 Uiso 1 1 calc R . .
H62B H 0.2749 -0.0708 0.5112 0.041 Uiso 1 1 calc R . .
H62C H 0.2009 -0.0990 0.5437 0.041 Uiso 1 1 calc R . .
O71 O 0.02329(11) 0.09803(8) 0.58428(8) 0.0186(3) Uani 1 1 d . . .
C72 C -0.02651(18) 0.09102(13) 0.63145(14) 0.0272(5) Uani 1 1 d . . .
H72A H -0.0797 0.0604 0.6106 0.041 Uiso 1 1 calc R . .
H72B H -0.0509 0.1340 0.6387 0.041 Uiso 1 1 calc R . .
H72C H 0.0167 0.0738 0.6775 0.041 Uiso 1 1 calc R . .
O1 O 0.29633(10) 0.04725(8) 0.43925(8) 0.0181(3) Uani 1 1 d . . .
C2 C 0.25179(15) 0.03640(11) 0.36965(11) 0.0183(4) Uani 1 1 d . A .
C3 C 0.29785(16) 0.01517(12) 0.32357(12) 0.0227(4) Uani 1 1 d . . .
C4 C 0.23939(18) 0.00231(12) 0.25369(12) 0.0252(4) Uani 1 1 d . A .
H4 H 0.2682 -0.0119 0.2216 0.030 Uiso 1 1 calc R . .
C5 C 0.13979(17) 0.00892(11) 0.22685(12) 0.0229(4) Uani 1 1 d D . .
C6 C 0.09637(16) 0.03302(11) 0.27173(11) 0.0196(4) Uani 1 1 d . A .
H6 H 0.0296 0.0399 0.2542 0.024 Uiso 1 1 calc R . .
C7 C 0.15217(15) 0.04694(10) 0.34295(11) 0.0171(4) Uani 1 1 d . . .
O8 O 0.12007(10) 0.06779(8) 0.39247(8) 0.0174(3) Uani 1 1 d . A .
C9 C 0.40562(18) 0.00608(14) 0.35182(14) 0.0296(5) Uani 1 1 d . . .
C10 C 0.45590(19) 0.07061(16) 0.38397(16) 0.0358(6) Uani 1 1 d . . .
H10A H 0.4385 0.1047 0.3469 0.054 Uiso 1 1 calc R . .
H10B H 0.5248 0.0639 0.4024 0.054 Uiso 1 1 calc R . .
H10C H 0.4365 0.0844 0.4231 0.054 Uiso 1 1 calc R . .
C11 C 0.4337(2) -0.04822(15) 0.40852(16) 0.0364(6) Uani 1 1 d . . .
H11A H 0.4157 -0.0351 0.4486 0.055 Uiso 1 1 calc R . .
H11B H 0.5025 -0.0552 0.4258 0.055 Uiso 1 1 calc R . .
H11C H 0.4009 -0.0891 0.3875 0.055 Uiso 1 1 calc R . .
C12 C 0.4403(2) -0.01436(19) 0.29234(16) 0.0442(8) Uani 1 1 d . . .
H12A H 0.4120 -0.0568 0.2724 0.066 Uiso 1 1 calc R . .
H12B H 0.5096 -0.0183 0.3121 0.066 Uiso 1 1 calc R . .
H12C H 0.4213 0.0190 0.2545 0.066 Uiso 1 1 calc R . .
C13 C 0.0765(5) -0.0114(3) 0.1498(4) 0.0226(6) Uani 0.473(3) 1 d PD A 1
C14 C -0.0310(4) -0.0095(4) 0.1318(3) 0.0393(10) Uani 0.473(3) 1 d PD A 1
H14A H -0.0465 -0.0363 0.1665 0.059 Uiso 0.473(3) 1 calc PR A 1
H14B H -0.0642 -0.0272 0.0835 0.059 Uiso 0.473(3) 1 calc PR A 1
H14C H -0.0511 0.0360 0.1338 0.059 Uiso 0.473(3) 1 calc PR A 1
C15 C 0.1011(5) -0.0827(3) 0.1362(3) 0.0378(9) Uani 0.473(3) 1 d PD A 1
H15A H 0.1678 -0.0850 0.1412 0.057 Uiso 0.473(3) 1 calc PR A 1
H15B H 0.0603 -0.0961 0.0877 0.057 Uiso 0.473(3) 1 calc PR A 1
H15C H 0.0907 -0.1122 0.1711 0.057 Uiso 0.473(3) 1 calc PR A 1
C16 C 0.1016(5) 0.0345(3) 0.0990(3) 0.0345(8) Uani 0.473(3) 1 d PD A 1
H16A H 0.0883 0.0801 0.1080 0.052 Uiso 0.473(3) 1 calc PR A 1
H16B H 0.0634 0.0228 0.0493 0.052 Uiso 0.473(3) 1 calc PR A 1
H16C H 0.1692 0.0299 0.1072 0.052 Uiso 0.473(3) 1 calc PR A 1
C91 C -0.2567(2) 0.11986(18) 0.1440(2) 0.0546(9) Uani 0.637(19) 1 d PD B 1
H91A H -0.3112 0.1436 0.1089 0.066 Uiso 0.637(19) 1 calc PR B 1
H91B H -0.2588 0.1271 0.1920 0.066 Uiso 0.637(19) 1 calc PR B 1
C92 C -0.2688(9) 0.0455(4) 0.1268(10) 0.086(4) Uani 0.637(19) 1 d PD B 1
H92A H -0.2733 0.0381 0.0775 0.129 Uiso 0.637(19) 1 calc PR B 1
H92B H -0.3268 0.0296 0.1321 0.129 Uiso 0.637(19) 1 calc PR B 1
H92C H -0.2139 0.0215 0.1598 0.129 Uiso 0.637(19) 1 calc PR B 1
C13' C 0.0855(5) -0.0088(3) 0.1484(4) 0.0226(6) Uani 0.527(3) 1 d PD A 2
C14' C 0.0011(4) -0.0515(3) 0.1456(3) 0.0393(10) Uani 0.527(3) 1 d PD A 2
H14D H 0.0241 -0.0896 0.1771 0.059 Uiso 0.527(3) 1 calc PR A 2
H14E H -0.0330 -0.0666 0.0964 0.059 Uiso 0.527(3) 1 calc PR A 2
H14F H -0.0420 -0.0256 0.1615 0.059 Uiso 0.527(3) 1 calc PR A 2
C15' C 0.1437(4) -0.0474(3) 0.1129(3) 0.0378(9) Uani 0.527(3) 1 d PD A 2
H15D H 0.1943 -0.0192 0.1095 0.057 Uiso 0.527(3) 1 calc PR A 2
H15E H 0.1020 -0.0613 0.0648 0.057 Uiso 0.527(3) 1 calc PR A 2
H15F H 0.1719 -0.0863 0.1418 0.057 Uiso 0.527(3) 1 calc PR A 2
C16' C 0.0507(4) 0.0550(3) 0.1066(3) 0.0345(8) Uani 0.527(3) 1 d PD A 2
H16D H 0.0078 0.0778 0.1252 0.052 Uiso 0.527(3) 1 calc PR A 2
H16E H 0.0168 0.0448 0.0559 0.052 Uiso 0.527(3) 1 calc PR A 2
H16F H 0.1053 0.0833 0.1120 0.052 Uiso 0.527(3) 1 calc PR A 2
C91' C -0.2567(2) 0.11986(18) 0.1440(2) 0.0546(9) Uani 0.363(19) 1 d P B 2
H91C H -0.3055 0.1547 0.1344 0.066 Uiso 0.363(19) 1 calc PR B 2
H91D H -0.2450 0.1014 0.1920 0.066 Uiso 0.363(19) 1 calc PR B 2
C92' C -0.2937(16) 0.0647(10) 0.0868(13) 0.086(4) Uani 0.363(19) 1 d PD B 2
H92D H -0.3049 0.0829 0.0393 0.129 Uiso 0.363(19) 1 calc PR B 2
H92E H -0.3533 0.0469 0.0877 0.129 Uiso 0.363(19) 1 calc PR B 2
H92F H -0.2464 0.0295 0.0973 0.129 Uiso 0.363(19) 1 calc PR B 2
O21 O -0.00172(11) 0.23924(8) 0.57261(8) 0.0210(3) Uani 1 1 d . . .
C22 C -0.08221(16) 0.25203(11) 0.51883(12) 0.0210(4) Uani 1 1 d . . .
C23 C -0.14850(18) 0.30089(13) 0.52062(13) 0.0270(5) Uani 1 1 d . . .
C24 C -0.22938(18) 0.30663(14) 0.45962(14) 0.0295(5) Uani 1 1 d . . .
H24 H -0.2746 0.3392 0.4591 0.035 Uiso 1 1 calc R . .
C25 C -0.24960(17) 0.26699(13) 0.39727(13) 0.0258(5) Uani 1 1 d . . .
C26 C -0.18353(15) 0.22031(12) 0.39613(12) 0.0211(4) Uani 1 1 d . . .
H26 H -0.1947 0.1936 0.3550 0.025 Uiso 1 1 calc R . .
C27 C -0.10041(15) 0.21326(11) 0.45642(12) 0.0197(4) Uani 1 1 d . . .
O28 O -0.03329(11) 0.16989(8) 0.46197(8) 0.0196(3) Uani 1 1 d . . .
C29 C -0.1284(2) 0.34473(16) 0.58678(15) 0.0374(6) Uani 1 1 d . . .
C30 C -0.1266(2) 0.30168(19) 0.64964(15) 0.0429(7) Uani 1 1 d . . .
H30A H -0.1142 0.3292 0.6921 0.064 Uiso 1 1 calc R . .
H30B H -0.0764 0.2686 0.6595 0.064 Uiso 1 1 calc R . .
H30C H -0.1881 0.2797 0.6375 0.064 Uiso 1 1 calc R . .
C31 C -0.0330(3) 0.38029(16) 0.60474(18) 0.0444(7) Uani 1 1 d . . .
H31A H -0.0349 0.4070 0.5637 0.067 Uiso 1 1 calc R . .
H31B H 0.0181 0.3478 0.6155 0.067 Uiso 1 1 calc R . .
H31C H -0.0214 0.4088 0.6464 0.067 Uiso 1 1 calc R . .
C32 C -0.2068(3) 0.3965(2) 0.5741(2) 0.0651(12) Uani 1 1 d . . .
H32A H -0.2677 0.3743 0.5644 0.098 Uiso 1 1 calc R . .
H32B H -0.2110 0.4239 0.5330 0.098 Uiso 1 1 calc R . .
H32C H -0.1917 0.4241 0.6168 0.098 Uiso 1 1 calc R . .
C33 C -0.33962(18) 0.27929(16) 0.33209(14) 0.0328(6) Uani 1 1 d . . .
C34 C -0.35264(18) 0.22965(15) 0.27227(14) 0.0336(6) Uani 1 1 d . . .
H34A H -0.2982 0.2320 0.2573 0.050 Uiso 1 1 calc R . .
H34B H -0.4110 0.2399 0.2314 0.050 Uiso 1 1 calc R . .
H34C H -0.3571 0.1852 0.2896 0.050 Uiso 1 1 calc R . .
C35 C -0.3333(3) 0.34884(17) 0.30436(17) 0.0460(8) Uani 1 1 d . . .
H35A H -0.3286 0.3811 0.3417 0.069 Uiso 1 1 calc R . .
H35B H -0.3903 0.3578 0.2619 0.069 Uiso 1 1 calc R . .
H35C H -0.2770 0.3520 0.2917 0.069 Uiso 1 1 calc R . .
C36 C -0.4277(2) 0.2744(2) 0.35282(18) 0.0574(11) Uani 1 1 d . . .
H36A H -0.4319 0.2299 0.3701 0.086 Uiso 1 1 calc R . .
H36B H -0.4850 0.2839 0.3108 0.086 Uiso 1 1 calc R . .
H36C H -0.4220 0.3064 0.3906 0.086 Uiso 1 1 calc R . .
S40 S 0.16884(4) 0.22525(3) 0.45106(3) 0.01977(10) Uani 1 1 d . . .
O41 O 0.24503(11) 0.17349(8) 0.47032(8) 0.0203(3) Uani 1 1 d . . .
O42 O 0.08300(11) 0.19759(8) 0.39336(8) 0.0201(3) Uani 1 1 d . . .
O43 O 0.14413(12) 0.23914(8) 0.51527(8) 0.0218(3) Uani 1 1 d . . .
O44 O 0.20099(13) 0.28410(9) 0.42795(10) 0.0276(4) Uani 1 1 d . . .
N80 N -0.06470(14) 0.25610(10) 0.17836(10) 0.0230(4) Uani 1 1 d . . .
C81 C -0.06519(19) 0.27567(14) 0.10497(13) 0.0300(5) Uani 1 1 d . . .
H81A H -0.1277 0.2959 0.0778 0.036 Uiso 1 1 calc R . .
H81B H -0.0167 0.3104 0.1125 0.036 Uiso 1 1 calc R . .
C82 C -0.0474(3) 0.22330(17) 0.05772(18) 0.0502(8) Uani 1 1 d . . .
H82A H -0.1051 0.1961 0.0356 0.060 Uiso 1 1 calc R . .
H82B H 0.0050 0.1941 0.0869 0.060 Uiso 1 1 calc R . .
C83 C -0.0210(2) 0.2565(2) -0.00120(16) 0.0505(9) Uani 1 1 d . . .
H83A H -0.0338 0.2257 -0.0418 0.061 Uiso 1 1 calc R . .
H83B H -0.0611 0.2959 -0.0190 0.061 Uiso 1 1 calc R . .
C84 C 0.0839(4) 0.2766(3) 0.0269(3) 0.095(2) Uani 1 1 d . . .
H84A H 0.0976 0.3048 0.0690 0.143 Uiso 1 1 calc R . .
H84B H 0.0972 0.3007 -0.0105 0.143 Uiso 1 1 calc R . .
H84C H 0.1238 0.2371 0.0400 0.143 Uiso 1 1 calc R . .
C85 C -0.06864(19) 0.32152(12) 0.21462(13) 0.0263(5) Uani 1 1 d . . .
H85A H -0.0157 0.3494 0.2135 0.032 Uiso 1 1 calc R . .
H85B H -0.1285 0.3440 0.1856 0.032 Uiso 1 1 calc R . .
C86 C -0.0631(2) 0.31833(12) 0.29159(13) 0.0281(5) Uani 1 1 d . . .
H86A H -0.0091 0.2902 0.3203 0.034 Uiso 1 1 calc R . .
H86B H -0.1222 0.2988 0.2930 0.034 Uiso 1 1 calc R . .
C87 C -0.0500(3) 0.38755(14) 0.32293(16) 0.0402(7) Uani 1 1 d . . .
H87A H -0.1055 0.4148 0.2949 0.048 Uiso 1 1 calc R . .
H87B H 0.0071 0.4076 0.3186 0.048 Uiso 1 1 calc R . .
C88 C -0.0391(3) 0.38790(16) 0.40141(17) 0.0439(7) Uani 1 1 d . . .
H88A H -0.0963 0.3693 0.4058 0.066 Uiso 1 1 calc R . .
H88B H -0.0303 0.4332 0.4194 0.066 Uiso 1 1 calc R . .
H88C H 0.0163 0.3614 0.4295 0.066 Uiso 1 1 calc R . .
C89 C -0.15266(17) 0.21729(13) 0.17321(15) 0.0301(5) Uani 1 1 d . B .
H89A H -0.1536 0.2143 0.2220 0.036 Uiso 1 1 calc R . .
H89B H -0.2088 0.2435 0.1442 0.036 Uiso 1 1 calc R . .
C90 C -0.1660(2) 0.14940(17) 0.1428(2) 0.0479(8) Uani 1 1 d . . .
H90A H -0.1114 0.1215 0.1711 0.057 Uiso 1 1 calc R B 1
H90B H -0.1687 0.1509 0.0929 0.057 Uiso 1 1 calc R B 1
C93 C 0.02420(16) 0.21784(11) 0.22135(12) 0.0221(4) Uani 1 1 d . . .
H93A H 0.0178 0.2020 0.2659 0.027 Uiso 1 1 calc R . .
H93B H 0.0282 0.1786 0.1934 0.027 Uiso 1 1 calc R . .
C94 C 0.11644(17) 0.25602(12) 0.24132(13) 0.0257(5) Uani 1 1 d . . .
H94A H 0.1206 0.2886 0.2790 0.031 Uiso 1 1 calc R . .
H94B H 0.1174 0.2803 0.1989 0.031 Uiso 1 1 calc R . .
C95 C 0.20166(18) 0.20962(13) 0.26850(14) 0.0291(5) Uani 1 1 d . . .
H95A H 0.2008 0.1800 0.2292 0.035 Uiso 1 1 calc R . .
H95B H 0.1968 0.1821 0.3076 0.035 Uiso 1 1 calc R . .
C96 C 0.2953(2) 0.24762(17) 0.29604(17) 0.0389(6) Uani 1 1 d . . .
H96A H 0.2995 0.2758 0.2578 0.058 Uiso 1 1 calc R . .
H96B H 0.3485 0.2165 0.3110 0.058 Uiso 1 1 calc R . .
H96C H 0.2981 0.2749 0.3369 0.058 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O51 1.5984(16) . ?
V1 O1 1.8680(15) . ?
V1 O56 1.9256(15) . ?
V1 O61 1.9879(16) . ?
V1 O41 2.0179(17) . ?
V1 O8 2.2321(15) . ?
V1 V4 3.0681(5) . ?
V2 O52 1.5902(16) . ?
V2 O55 1.9362(15) 3_556 ?
V2 O28 1.9673(16) . ?
V2 O8 1.9708(15) . ?
V2 O42 2.0504(16) . ?
V2 O56 2.4001(15) . ?
V3 O53 1.5945(16) . ?
V3 O21 1.8787(16) . ?
V3 O56 1.9402(15) . ?
V3 O71 1.9745(16) . ?
V3 O43 2.0208(16) . ?
V3 O28 2.2225(16) . ?
V3 V4 3.0443(6) . ?
V4 O54 1.5944(16) . ?
V4 O55 1.7120(15) . ?
V4 O71 1.9556(16) . ?
V4 O61 1.9820(15) . ?
V4 O56 2.0234(15) . ?
O55 V2 1.9361(15) 3_556 ?
O61 C62 1.429(3) . ?
O71 C72 1.424(3) . ?
O1 C2 1.328(2) . ?
C2 C7 1.419(3) . ?
C2 C3 1.420(3) . ?
C3 C4 1.380(3) . ?
C3 C9 1.529(3) . ?
C4 C5 1.409(3) . ?
C5 C6 1.391(3) . ?
C5 C13' 1.529(8) . ?
C5 C13 1.546(8) . ?
C6 C7 1.396(3) . ?
C7 O8 1.331(2) . ?
C9 C11 1.530(4) . ?
C9 C12 1.533(4) . ?
C9 C10 1.534(4) . ?
C13 C16 1.533(7) . ?
C13 C14 1.534(7) . ?
C13 C15 1.546(7) . ?
C91 C90 1.510(5) . ?
C91 C92 1.547(8) . ?
C13' C16' 1.528(7) . ?
C13' C14' 1.530(7) . ?
C13' C15' 1.542(7) . ?
O21 C22 1.322(3) . ?
C22 C27 1.420(3) . ?
C22 C23 1.423(3) . ?
C23 C24 1.380(4) . ?
C23 C29 1.536(4) . ?
C24 C25 1.426(4) . ?
C25 C26 1.386(3) . ?
C25 C33 1.521(3) . ?
C26 C27 1.394(3) . ?
C27 O28 1.320(3) . ?
C29 C30 1.531(5) . ?
C29 C31 1.535(5) . ?
C29 C32 1.536(4) . ?
C33 C34 1.527(4) . ?
C33 C35 1.536(5) . ?
C33 C36 1.544(4) . ?
S40 O44 1.4330(18) . ?
S40 O42 1.4949(17) . ?
S40 O43 1.5008(17) . ?
S40 O41 1.5030(17) . ?
N80 C93 1.518(3) . ?
N80 C89 1.520(3) . ?
N80 C81 1.528(3) . ?
N80 C85 1.529(3) . ?
C81 C82 1.517(4) . ?
C82 C83 1.541(5) . ?
C83 C84 1.531(6) . ?
C85 C86 1.522(3) . ?
C86 C87 1.524(4) . ?
C87 C88 1.526(4) . ?
C89 C90 1.493(4) . ?
C93 C94 1.517(3) . ?
C94 C95 1.527(3) . ?
C95 C96 1.528(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O51 V1 O1 97.53(7) . . ?
O51 V1 O56 109.10(7) . . ?
O1 V1 O56 153.32(7) . . ?
O51 V1 O61 97.27(8) . . ?
O1 V1 O61 98.94(7) . . ?
O56 V1 O61 76.66(6) . . ?
O51 V1 O41 97.15(8) . . ?
O1 V1 O41 92.89(7) . . ?
O56 V1 O41 85.49(6) . . ?
O61 V1 O41 159.95(6) . . ?
O51 V1 O8 172.16(7) . . ?
O1 V1 O8 75.14(6) . . ?
O56 V1 O8 78.18(6) . . ?
O61 V1 O8 81.35(6) . . ?
O41 V1 O8 86.17(6) . . ?
O51 V1 V4 95.45(6) . . ?
O1 V1 V4 137.66(5) . . ?
O56 V1 V4 40.18(5) . . ?
O61 V1 V4 39.32(4) . . ?
O41 V1 V4 125.15(5) . . ?
O8 V1 V4 88.36(4) . . ?
O52 V2 O55 102.70(8) . 3_556 ?
O52 V2 O28 107.23(8) . . ?
O55 V2 O28 89.38(7) 3_556 . ?
O52 V2 O8 106.88(8) . . ?
O55 V2 O8 91.06(6) 3_556 . ?
O28 V2 O8 144.90(6) . . ?
O52 V2 O42 97.36(8) . . ?
O55 V2 O42 159.89(6) 3_556 . ?
O28 V2 O42 83.42(7) . . ?
O8 V2 O42 84.28(7) . . ?
O52 V2 O56 178.76(7) . . ?
O55 V2 O56 76.06(6) 3_556 . ?
O28 V2 O56 72.76(6) . . ?
O8 V2 O56 73.32(6) . . ?
O42 V2 O56 83.87(6) . . ?
O53 V3 O21 98.70(8) . . ?
O53 V3 O56 108.25(8) . . ?
O21 V3 O56 152.96(7) . . ?
O53 V3 O71 99.60(8) . . ?
O21 V3 O71 97.29(7) . . ?
O56 V3 O71 76.44(6) . . ?
O53 V3 O43 96.68(8) . . ?
O21 V3 O43 93.90(7) . . ?
O56 V3 O43 85.31(6) . . ?
O71 V3 O43 158.58(7) . . ?
O53 V3 O28 174.15(8) . . ?
O21 V3 O28 75.55(6) . . ?
O56 V3 O28 77.46(6) . . ?
O71 V3 O28 80.31(6) . . ?
O43 V3 O28 84.89(6) . . ?
O53 V3 V4 95.23(7) . . ?
O21 V3 V4 135.95(5) . . ?
O56 V3 V4 40.83(4) . . ?
O71 V3 V4 39.01(5) . . ?
O43 V3 V4 125.69(5) . . ?
O28 V3 V4 88.36(4) . . ?
O54 V4 O55 104.68(8) . . ?
O54 V4 O71 98.72(8) . . ?
O55 V4 O71 98.88(7) . . ?
O54 V4 O61 97.31(8) . . ?
O55 V4 O61 102.51(7) . . ?
O71 V4 O61 148.96(7) . . ?
O54 V4 O56 110.13(8) . . ?
O55 V4 O56 145.17(7) . . ?
O71 V4 O56 74.97(6) . . ?
O61 V4 O56 74.61(6) . . ?
O54 V4 V3 96.22(6) . . ?
O55 V4 V3 136.36(5) . . ?
O71 V4 V3 39.45(5) . . ?
O61 V4 V3 112.40(5) . . ?
O56 V4 V3 38.83(4) . . ?
O54 V4 V1 96.55(6) . . ?
O55 V4 V1 139.14(5) . . ?
O71 V4 V1 112.06(5) . . ?
O61 V4 V1 39.46(5) . . ?
O56 V4 V1 37.88(4) . . ?
V3 V4 V1 73.321(13) . . ?
V4 O55 V2 149.88(9) . 3_556 ?
V1 O56 V3 141.50(8) . . ?
V1 O56 V4 101.93(7) . . ?
V3 O56 V4 100.34(7) . . ?
V1 O56 V2 100.88(6) . . ?
V3 O56 V2 101.20(6) . . ?
V4 O56 V2 108.63(6) . . ?
C62 O61 V4 120.17(14) . . ?
C62 O61 V1 120.68(13) . . ?
V4 O61 V1 101.22(7) . . ?
C72 O71 V4 122.76(15) . . ?
C72 O71 V3 128.06(14) . . ?
V4 O71 V3 101.54(7) . . ?
C2 O1 V1 124.14(13) . . ?
O1 C2 C7 115.23(18) . . ?
O1 C2 C3 123.99(19) . . ?
C7 C2 C3 120.78(19) . . ?
C4 C3 C2 116.0(2) . . ?
C4 C3 C9 123.3(2) . . ?
C2 C3 C9 120.8(2) . . ?
C3 C4 C5 124.3(2) . . ?
C6 C5 C4 118.9(2) . . ?
C6 C5 C13' 123.5(3) . . ?
C4 C5 C13' 117.6(3) . . ?
C6 C5 C13 118.6(3) . . ?
C4 C5 C13 122.4(3) . . ?
C13' C5 C13 5.8(5) . . ?
C5 C6 C7 119.1(2) . . ?
O8 C7 C6 125.65(19) . . ?
O8 C7 C2 113.52(18) . . ?
C6 C7 C2 120.76(19) . . ?
C7 O8 V2 140.09(13) . . ?
C7 O8 V1 111.85(12) . . ?
V2 O8 V1 105.47(7) . . ?
C3 C9 C11 109.1(2) . . ?
C3 C9 C12 111.8(2) . . ?
C11 C9 C12 107.8(2) . . ?
C3 C9 C10 110.4(2) . . ?
C11 C9 C10 110.2(2) . . ?
C12 C9 C10 107.5(2) . . ?
C16 C13 C14 109.5(6) . . ?
C16 C13 C15 108.5(6) . . ?
C14 C13 C15 106.6(6) . . ?
C16 C13 C5 106.9(5) . . ?
C14 C13 C5 116.0(5) . . ?
C15 C13 C5 109.1(5) . . ?
C90 C91 C92 114.7(5) . . ?
C16' C13' C5 108.1(4) . . ?
C16' C13' C14' 110.4(5) . . ?
C5 C13' C14' 107.0(5) . . ?
C16' C13' C15' 108.5(5) . . ?
C5 C13' C15' 114.7(5) . . ?
C14' C13' C15' 108.1(5) . . ?
C22 O21 V3 123.06(14) . . ?
O21 C22 C27 115.59(19) . . ?
O21 C22 C23 124.2(2) . . ?
C27 C22 C23 120.2(2) . . ?
C24 C23 C22 116.0(2) . . ?
C24 C23 C29 123.1(2) . . ?
C22 C23 C29 120.8(2) . . ?
C23 C24 C25 124.4(2) . . ?
C26 C25 C24 118.8(2) . . ?
C26 C25 C33 121.3(2) . . ?
C24 C25 C33 119.8(2) . . ?
C25 C26 C27 118.7(2) . . ?
O28 C27 C26 124.1(2) . . ?
O28 C27 C22 113.95(19) . . ?
C26 C27 C22 121.9(2) . . ?
C27 O28 V2 139.46(14) . . ?
C27 O28 V3 111.73(13) . . ?
V2 O28 V3 106.78(7) . . ?
C30 C29 C31 110.5(3) . . ?
C30 C29 C23 108.8(3) . . ?
C31 C29 C23 110.1(2) . . ?
C30 C29 C32 107.6(3) . . ?
C31 C29 C32 108.7(3) . . ?
C23 C29 C32 111.2(2) . . ?
C25 C33 C34 112.5(2) . . ?
C25 C33 C35 107.9(2) . . ?
C34 C33 C35 109.2(2) . . ?
C25 C33 C36 110.2(2) . . ?
C34 C33 C36 107.5(3) . . ?
C35 C33 C36 109.5(3) . . ?
O44 S40 O42 111.39(10) . . ?
O44 S40 O43 110.30(10) . . ?
O42 S40 O43 108.40(9) . . ?
O44 S40 O41 110.25(10) . . ?
O42 S40 O41 107.52(9) . . ?
O43 S40 O41 108.90(9) . . ?
S40 O41 V1 128.05(9) . . ?
S40 O42 V2 126.32(9) . . ?
S40 O43 V3 128.16(10) . . ?
C93 N80 C89 110.12(18) . . ?
C93 N80 C81 111.62(18) . . ?
C89 N80 C81 112.4(2) . . ?
C93 N80 C85 110.95(18) . . ?
C89 N80 C85 107.13(19) . . ?
C81 N80 C85 104.39(18) . . ?
C82 C81 N80 119.1(2) . . ?
C81 C82 C83 109.5(3) . . ?
C84 C83 C82 111.3(3) . . ?
C86 C85 N80 116.89(19) . . ?
C85 C86 C87 109.4(2) . . ?
C86 C87 C88 112.3(2) . . ?
C90 C89 N80 119.3(2) . . ?
C89 C90 C91 110.2(3) . . ?
C94 C93 N80 115.14(19) . . ?
C93 C94 C95 110.7(2) . . ?
C94 C95 C96 111.5(2) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        33.07
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.898
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.097
_database_code_depnum_ccdc_archive 'CCDC 981750'
